CN106511133B - Essential oil nano-particles, preparation method thereof and application thereof in preparing mosquito-repellent products - Google Patents
Essential oil nano-particles, preparation method thereof and application thereof in preparing mosquito-repellent products Download PDFInfo
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Abstract
The invention relates to the technical field of daily chemicals, in particular to an essential oil nano-particle, a preparation method thereof and application thereof in preparing mosquito repellent products. The plant essential oil is used as the mosquito repellent, and the mosquito repellent effect is good through the synergistic and mutual promotion effects of the plant essential oils. In addition, various essential oils are coated by the mesoporous silicon dioxide, so that the essential oils are more stable and have a slow release effect. The microsphere can be added into mosquito repellent product, so as to reduce the addition amount of essential oil in mosquito repellent emulsion and prolong its action time. The essential oil, the vegetable oil and the purslane extract in the mosquito repellent emulsion provided by the invention also have the effects of anti-allergy, anti-inflammation, itching relieving and swelling diminishing, and the irritation to the skin is reduced, so that the mosquito repellent emulsion has better safety and more efficient mosquito repellent effect. Experiments show that under a proper proportion, the effective mosquito repelling time of the mosquito repelling emulsion provided by the invention can reach 14.1 h; the effective avoidance rate can still reach 87.3 percent after 18 hours.
Description
Technical Field
The invention relates to the technical field of daily chemicals, in particular to an essential oil nano-particle, a preparation method thereof and application thereof in preparing mosquito repellent products.
Background
The variety of the mosquitoes is many, more than 3000 mosquitoes exist in the world, wherein more than 300 mosquitoes exist in China, the mosquitoes are widely distributed, and the three types of mosquitoes, namely anopheles, culex and aedes are common. Although the mosquitoes are small, the mosquitoes cause little damage, and are common harmful insects in summer and autumn. Mosquitoes not only bite and suck blood to cause pruritus, but also transmit a plurality of diseases, such as malaria, epidemic encephalitis B, filariasis, dengue fever, yellow fever and the like. As a vector for transmitting diseases, human beings have recognized the importance of mosquito control, and since the 40 th century of the 20 th century, some highly effective insecticides such as hexachlorocyclohexane (hexachlorocyclohexane), bis-p-chlorophenyl trichloroethane (dichlorodiphenyl ethane) and the like have been widely used to eradicate malaria. However, with the long-term and wide use of these insecticides, there are increasing problems of mosquito resistance, insecticide contamination of the environment, etc., such as "three R" problems, i.e., residue (residual), resistance (resistance) and rampant (resurgence) of insect pests. More importantly, the chemical components can be absorbed by the human body through the skin, thus seriously harming the health of human beings. In recent years, with the development of society and the increasing improvement of human life quality, it is important to find a natural mosquito repellent product with small toxic and side effect, safety, environmental protection and easy degradation for insect prevention and killing. At present, the plant volatile oil is used as a natural mosquito repellent to gradually replace a chemical insecticide, has certain poisoning and repelling effects on mosquitoes, and has the potential of developing the plant volatile oil into a new generation of mosquito killing agent and mosquito repellent.
Essential oil is a general name of volatile oily components which are present in plants, have aromatic odor, can be distilled with water vapor and are immiscible with water, is widely distributed in traditional Chinese medicinal materials, mainly contains micromolecular terpenoid compounds and has various effects, so that the application of the essential oil is more and more emphasized, particularly in the aspect of mosquito repelling. Plants are applied to mosquito repelling and mosquito killing for a long time, and in order to prevent the invasion of mosquitoes, ancient people usually can cultivate some mosquito-repelling plants at home, such as mozzie buster, wrinkled gianthyssop herb, violet, lavender and the like, and the flowers can repel mosquitoes and purify air. The experience of burning mugwort to fumigate and kill and repel mosquitoes in summer and evening is recorded in China before the yuan. The hanging sachet is also one of the living habits of ancient people, and medicinal materials in a plurality of sachets also have the mosquito repelling effect, such as agastache rugosus, mint, star anise, fennel and the like. In the southwest region, mosquito bite is prevented by applying juice of Eucalyptus globulus Labill. In western regions of south africa, mosquito repelling and killing plants mainly include Meliaceae and Anacardiaceae, such as bur hard walnut Sclerocarya birrea l, melia meliaca zedarach l, and nasturtium erica emetica l. Researches show that the citronella essential oil, the tea tree essential oil, the lavender essential oil, the cedar essential oil, the eucalyptus leaf essential oil, the argy wormwood leaf essential oil, the cinnamomum camphora leaf essential oil, the mint essential oil, the cinnamon essential oil and the clove essential oil have the mosquito repelling effect.
However, the plant essential oil is a mixture of various chemical components, has no fixed boiling point and freezing point, is very easily influenced by external environmental conditions (such as illumination, temperature, humidity and the like), has very unstable properties, is easy to disperse, deteriorate, dissipate and volatilize, and is greatly restricted in development and application. The sustained and controlled release technology is one of effective means for effectively solving the problems of unstable essential oil, short efficacy period and the like. Therefore, the development of a sustained-release formulation suitable for essential oil and the application of the sustained-release formulation in the preparation of mosquito repellent agents become the focus of current research.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide an essential oil nanoparticle, a preparation method thereof, and an application thereof in preparing a mosquito repellent product.
The invention provides essential oil nanoparticles, which are prepared from the following raw materials in parts by mass:
in an embodiment of the invention, the essential oil is selected from catnip essential oil, cinnamon essential oil, rosemary essential oil, chestnut flower essential oil, corolla fumigated leaf essential oil, galangal essential oil, parthenolide essential oil, thyme essential oil, lantana camara essential oil or tea tree essential oil.
The preparation method of the essential oil provided by the invention adopts a steam distillation method, which can be self-made or commercially available, and the implementation thereof is within the protection scope of the invention.
In some embodiments, the essential oil is a combination of catmint essential oil and cinnamon essential oil.
In this example, the mass ratio of catnip essential oil to cinnamon essential oil was 3: 2.
In some embodiments, the essential oil is a combination of rosemary essential oil, chestnut flower essential oil, corolla fumigated leaf essential oil, galangal essential oil, guayule essential oil, thyme essential oil, lantana essential oil, and tea tree essential oil.
In this example, the mass ratio of rosemary essential oil, chestnut flower essential oil, corolla fumigated leaf essential oil, galangal essential oil, guayule essential oil, thyme essential oil, lantana essential oil and tea tree essential oil is 2:18:10:5:20:3:12: 5.
In some embodiments, the essential oil is a combination of catnip essential oil, cinnamon essential oil, rosemary essential oil, chestnut flower essential oil, corolla fumigated leaf essential oil, galangal essential oil, parthenolide essential oil, thyme essential oil, lantana essential oil, and tea tree essential oil.
In this example, the mass ratio of the schizonepeta essential oil, the cinnamon essential oil, the rosemary essential oil, the chestnut flower essential oil, the corolla fumigated leaf essential oil, the galangal essential oil, the parthenolia essential oil, the thyme essential oil, the lantana essential oil and the tea tree essential oil is 12:15:3:20:10:3:10:5:15: 7.
In some embodiments, the essential oil is a combination of catnip essential oil, chestnut flower essential oil, corolla fumigated leaf essential oil, guayule essential oil, thyme essential oil, lantana essential oil, and tea tree essential oil.
In this example, the mass ratio of schizonepeta essential oil, chestnut flower essential oil, corolla fumigated leaf essential oil, silver cinerary chrysanthemum essential oil, thyme essential oil, lantana camara essential oil to tea tree essential oil is 10:8:12:10:4:13: 3.
In the invention, the preparation method of the essential oil nanoparticles comprises the following steps:
step 1: dissolving sucrose stearate and essential oil in water at 50-60 ℃, adding mesoporous silicon dioxide, and performing ultrasonic treatment for 0.5-1 h to prepare a dispersion liquid;
step 2: and dropwise adding a dextran quaternary ammonium salt water solution into the dispersion liquid, performing ultrasonic treatment for 5-10 min, centrifuging, collecting precipitate, washing and drying the precipitate to obtain the essential oil nanoparticles.
The preparation method of the mesoporous silica comprises the following steps:
dissolving cetyl trimethyl ammonium bromide in deionized water, mixing with NaOH solution, heating to 80 ℃, adding ethyl orthosilicate while stirring, and reacting for 6 hours; filtering to obtain a precipitate, dissolving the precipitate in methanol, dropwise adding concentrated hydrochloric acid, heating to 70 ℃, pickling for 18 hours, filtering, collecting the precipitate, washing with methanol and deionized water, and drying to obtain the mesoporous silica.
The concentration of the hexadecyl trimethyl ammonium bromide in the solution obtained by dissolving the hexadecyl trimethyl ammonium bromide in the deionized water is 0.05 g/mL.
The concentration of the NaOH solution is 2 mol/L.
The volume ratio of the NaOH solution to the cetyl trimethyl ammonium bromide solution is (56-122): 340-700.
The mass ratio of the ethyl orthosilicate to the hexadecyl trimethyl ammonium bromide is (87-174): (17-35).
Preferably, the mass ratio of ethyl orthosilicate to cetyltrimethylammonium bromide is 5: 1.
The concentration of the concentrated hydrochloric acid is 37.5%.
The mass-volume ratio of the precipitate to the concentrated hydrochloric acid is (25 g-50 g): 10 mL-20 mL.
In the embodiment of the invention, in the step 1:
the mass-volume ratio of the sucrose stearate to the water is (3 g-7 g): (80 mL-150 mL);
the mass-volume ratio of the essential oil to the water is (50 g-100 g): (80 mL-150 mL).
The mass ratio of the sucrose stearate to the essential oil is (3-7): (50-100).
The mass ratio of the mesoporous silicon dioxide to the essential oil is (25 g-50 g) to (50 g-100 g).
In the embodiment of the present invention, it is,
in the step 1, the frequency of the ultrasound is 40KHz, and the power is 200W;
in the step 2, the frequency of the ultrasound is 40KHz, and the power is 200W.
In the embodiment of the invention, the concentration of the quaternary ammonium salt of glucan in the aqueous solution of the quaternary ammonium salt of glucan in the step 2 is 0.5 g/mL;
the volume ratio of the dispersion liquid to the glucan quaternary ammonium salt water solution is (80-150): (100-200).
The concentration of the dextran quaternary ammonium salt water solution is 0.5 g/mL.
The rotation speed of the centrifugation in the step 2 is 10000rpm, and the time is 10 min.
The essential oil nanoparticles provided by the invention take mesoporous silicon dioxide as a carrier, various plant essential oils are adsorbed in a pore channel, and then negative charges of a silicon hydroxyl base band on the surface of the mesoporous silicon dioxide and a high polymer dextran quaternary ammonium salt with positive charges are compounded in an aqueous solution through positive and negative charges, so that the high polymer is wound on the surface of the mesoporous silicon dioxide to play a slow release role, the stability of the essential oil is improved, and the water solubility of the essential oil is also improved. The nano-particles can have a mosquito repelling effect, and the mosquito repelling effect is lasting.
The invention also provides application of the essential oil nanoparticles in preparation of mosquito repellent products.
The mosquito repelling product is mosquito repelling emulsion, mosquito repelling spray, mosquito repelling liquid, mosquito repelling tablet, mosquito repelling bracelet or mosquito repelling paste.
The mosquito-repellent emulsion provided by the invention comprises the essential oil nanoparticles provided by the invention, vegetable oil, purslane extract, glycerol, ascorbyl tetraisopalmitate, cetostearyl alcohol, laureth-23, a humectant, a thickener, a pH regulator and deionized water.
In the embodiment of the invention, the mosquito repellent emulsion comprises the following components in percentage by mass:
in an embodiment of the present invention, the vegetable oil is selected from jojoba oil, macadamia nut oil, evening primrose oil, sweet almond oil, wheat germ oil, coix seed oil, rice bran oil or carrot oil;
the humectant is selected from butanediol, hexanediol, sodium hyaluronate, β -dextran, allantoin or nicotinamide;
the thickening agent is selected from carbomer, seaweed gum, acacia gum, xanthan gum or Caesalpinia spinosa;
the pH regulator is selected from triethanolamine or citric acid.
In one specific embodiment, the mosquito repellent emulsion comprises the following components in percentage by mass:
40% of plant essential oil nanoparticles, 7% of jojoba oil, 1% of evening primrose oil, 1.5% of sweet almond oil, 2.7% of wheat germ oil, 2% of pearl barley oil, 0.8% of carrot oil, 6% of glycerol, 4% of butanediol, 0.5% of sodium hyaluronate, 1% of β -dextran, 0.5% of allantoin, 1% of purslane extract, 0.3% of ascorbyl tetraisopalmitate, 0.3% of carbomer, 4% of cetostearyl alcohol, 231% of laureth, 0.2% of triethanolamine and the balance of deionized water to 100%.
In this example, the essential oil in the plant essential oil nanoparticles is a combination of catnip essential oil and cinnamon essential oil.
In another specific embodiment, the mosquito repellent emulsion comprises the following components in percentage by mass:
30% of plant essential oil nanoparticles, 8% of macadamia nut oil, 9% of glycerol, 0.8% of hexanediol, 3.2% of β -glucan, 4% of purslane extract, 0.6% of ascorbyl tetraisopalmitate, 0.02% of seaweed gel, 0.08% of tara gum, 1% of cetostearyl alcohol, 232% of laureth, 0.05% of citric acid and the balance of deionized water to 100%.
In this embodiment, the essential oil in the plant essential oil nanoparticles is a combination of rosemary essential oil, chestnut flower essential oil, corolla fumigated leaf essential oil, galangal essential oil, guayule essential oil, thyme essential oil, lantana essential oil, and tea tree essential oil.
In another specific embodiment, the mosquito repellent emulsion comprises the following components in percentage by mass:
plant essential oil nanoparticles 20%, macadamia nut oil 4%, evening primrose oil 2%, wheat germ oil 1%, rice bran oil 3%, carrot oil 1.5%, glycerin 12%, niacinamide 2%, purslane extract 2.5%, ascorbyl tetraisopalmitate 1%, xanthan gum 0.1%, gum arabic 0.15%, cetostearyl alcohol 2.5%, laureth-233%, triethanolamine 0.08%, citric acid 0.05%, deionized water to 100%.
In this example, the essential oil is a combination of catnip essential oil, cinnamon essential oil, rosemary essential oil, chestnut flower essential oil, corolla fumigated leaf essential oil, galangal essential oil, guayule essential oil, thyme essential oil, lantana essential oil, and tea tree essential oil.
In another specific embodiment, the mosquito repellent emulsion comprises the following components in percentage by mass:
35% of plant essential oil nanoparticles, 5% of jojoba oil, 3% of wheat germ oil, 2% of carrot oil, 8% of glycerol, 1% of hexanediol and 1.2% of sodium hyaluronate
％0.8% of nicotinamide, 2% of purslane extract, 0.8% of ascorbyl tetraisopalmitate, 0.2% of tara gum, 2% of cetostearyl alcohol, 232% of laureth, 0.1% of triethanolamine, 0.05% of citric acid and the balance of deionized water.
In this example, the essential oil is a combination of catnip essential oil, chestnut flower essential oil, corolla fumigated leaf essential oil, guayule essential oil, thyme essential oil, lantana essential oil, and tea tree essential oil.
The preparation method of the mosquito-repellent emulsion provided by the invention comprises the following steps:
step 1: mixing vegetable oil, cetostearyl alcohol and laureth-23, stirring, heating to 70-85 ℃, stirring, and keeping the temperature for 5-10 min to obtain an oil phase;
step 2: mixing deionized water, a thickening agent and glycerol, stirring, heating to 70-85 ℃, stirring, and keeping the temperature for 5-10 min to obtain a water phase;
and step 3: adding the oil phase into the water phase under the condition of stirring, homogenizing for 2-5 min, stirring and cooling to 40-45 ℃; adjusting the pH value to 5-7, and sequentially adding the plant essential oil nanoparticles, ascorbyl tetraisopalmitate, humectant and purslane extract according to claim 1 or 2; cooling to obtain the mosquito repellent emulsion.
The plant essential oil is used as the mosquito repellent, and the mosquito repellent effect is good through the synergistic and mutual promotion effects of the plant essential oils. In addition, various essential oils are coated by the mesoporous silicon dioxide, so that the essential oil is more stable and has a slow release effect. The microsphere can be added into mosquito repellent product, so as to reduce the addition amount of essential oil in mosquito repellent emulsion and prolong its action time. The essential oil, the vegetable oil and the purslane extract in the mosquito repellent emulsion provided by the invention also have the effects of anti-allergy, anti-inflammation, itching relieving and swelling diminishing, and the irritation and permeability to the skin are reduced, so that the mosquito repellent emulsion has better safety and more efficient mosquito repellent effect. Experiments show that under a proper proportion, the effective mosquito repelling time of the mosquito repelling emulsion provided by the invention can reach 14.1 h; the effective avoidance rate can still reach 87.3 percent after 18 hours.
Detailed Description
The invention provides an essential oil nano-particle, a preparation method thereof and application thereof in preparing mosquito repellent products. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The materials adopted by the invention are all common commercial products and can be purchased in the market. .
Specifically, the preparation method of the essential oil provided by the invention comprises the following steps: mixing plant material with water, heating to boil, heating for 150min, collecting distillate under circulation of cold water for 20min, standing, and separating essential oil. The plant material may be chestnut flower, corolla fumigated leaf or parthenium cinerascens. Other plant materials are also possible.
According to the invention, the preparation methods of the Chinese chestnut flower essential oil, the small crown smoked leaf essential oil and the silver ash chrysanthemum essential oil are adopted, and the schizonepeta essential oil, the cinnamon essential oil, the thyme essential oil and the tea tree essential oil are purchased from Guangzhou Chengjingya trade company; rosemary oil was purchased from Mitsubishi trade, Guangzhou; galangal essential oil and lantana essential oil are purchased from Shanghai Paris trade company Limited.
The invention is further illustrated by the following examples:
example 1
Dissolving 17g of hexadecyl trimethyl ammonium bromide solution in 340mL of deionized water, performing ultrasonic treatment to completely dissolve the hexadecyl trimethyl ammonium bromide solution, then adding 56mL of NaOH solution (2M), heating to 80 ℃, adding 87g of ethyl orthosilicate while stirring, reacting for 6 hours, filtering, then dissolving in 60mL of methanol, dropwise adding 10mL of concentrated hydrochloric acid, heating to 70 ℃, pickling for 18 hours, filtering, collecting precipitate, washing with methanol and deionized water for multiple times, and drying to obtain 25g of mesoporous silica.
Dissolving 3g of sucrose stearate, 30g of schizonepeta essential oil and 20g of cinnamon essential oil in 80mL of 50 ℃ water, then adding 25g of mesoporous silica, performing ultrasonic treatment for 1h, then dropwise adding 100mL of glucan quaternary ammonium salt aqueous solution (0.5g/mL), performing ultrasonic treatment for 8min, centrifuging (10000rpm, 10min), washing with deionized water for multiple times, and drying to obtain 120g of nanoparticles.
Example 2
Dissolving 26g of hexadecyl trimethyl ammonium bromide solution in 520mL of deionized water, performing ultrasonic treatment to completely dissolve the hexadecyl trimethyl ammonium bromide solution, then adding 89mL of NaOH solution (2M), heating to 75 ℃, adding 130g of ethyl orthosilicate while stirring, reacting for 7h, filtering, then dissolving in 70mL of methanol, dropwise adding 15mL of concentrated hydrochloric acid, heating to 65 ℃, performing acid washing for 22h, filtering, collecting precipitate, washing with methanol and deionized water for multiple times, and drying to obtain 37g of mesoporous silica.
Dissolving 5g of sucrose stearate, 2g of rosemary essential oil, 18g of Chinese chestnut flower essential oil, 10g of corolla fumigating leaf essential oil, 5g of galangal essential oil, 20g of guayule essential oil, 3g of thyme essential oil, 12g of lantana essential oil and 5g of tea tree essential oil in 115mL of water at 55 ℃, adding 37g of mesoporous silicon dioxide, performing ultrasonic treatment for 0.5h, dropwise adding 150mL of glucan quaternary ammonium salt aqueous solution (0.5g/mL), performing ultrasonic treatment for 5min, centrifuging (11000rpm, 22min), washing with deionized water for multiple times, and drying to obtain 180g of nanoparticles.
Example 3
Dissolving 35g of hexadecyl trimethyl ammonium bromide solution in 700mL of deionized water, carrying out ultrasonic treatment to completely dissolve the hexadecyl trimethyl ammonium bromide solution, then adding 122mL of NaOH solution (2M), heating to 85 ℃, adding 174g of ethyl orthosilicate while stirring, reacting for 8 hours, filtering, then dissolving in 80mL of methanol, dropwise adding 20mL of concentrated hydrochloric acid, heating to 60 ℃, carrying out acid washing for 24 hours, filtering, collecting precipitate, washing with methanol and deionized water for multiple times, and drying to obtain 50g of mesoporous silica.
Dissolving 7g of sucrose stearate, 12g of schizonepeta essential oil, 15g of cinnamon essential oil, 3g of rosemary essential oil, 20g of Chinese chestnut flower essential oil, 10g of corolla fumigated leaf essential oil, 3g of galangal essential oil, 10g of parthenolide essential oil, 5g of thyme essential oil, 15g of lantana essential oil and 7g of tea tree essential oil in 150mL of 60 ℃ water, adding 50g of mesoporous silicon dioxide, performing ultrasonic treatment for 1h, dropwise adding 200mL of glucan quaternary ammonium salt water solution (0.5g/mL), performing ultrasonic treatment for 10min, centrifuging (12000rpm, 15min), washing with deionized water for multiple times, and drying to obtain 235g of nanoparticles.
Example 4
Dissolving 22g of hexadecyl trimethyl ammonium bromide solution in 240mL of deionized water, performing ultrasonic treatment to completely dissolve the hexadecyl trimethyl ammonium bromide solution, then adding 75mL of NaOH solution (2M), heating to 80 ℃, adding 110g of ethyl orthosilicate while stirring, reacting for 7h, filtering, dissolving in 68mL of methanol, dropwise adding 13mL of concentrated hydrochloric acid, heating to 60 ℃, performing acid washing for 20h, filtering, collecting precipitate, washing with methanol and deionized water for multiple times, and drying to obtain 31g of mesoporous silica.
Dissolving 4g of sucrose stearate, 10g of schizonepeta essential oil, 8g of Chinese chestnut flower essential oil, 12g of corolla fumigating leaf essential oil, 10g of guayule essential oil, 4g of thyme essential oil, 13g of lantana essential oil and 3g of tea tree essential oil in 100mL of water with the temperature of 55 ℃, adding 31g of mesoporous silicon dioxide, carrying out ultrasonic treatment for 0.5h, then dropwise adding 120mL of glucan quaternary ammonium salt aqueous solution (0.5g/mL), carrying out ultrasonic treatment for 7min, centrifuging (10000rpm and 12min), washing with deionized water for multiple times, and drying to obtain 145g of nanoparticles.
Example 5
Dissolving 6.8g of hexadecyl trimethyl ammonium bromide solution in 136mL of deionized water, carrying out ultrasonic treatment to completely dissolve the hexadecyl trimethyl ammonium bromide solution, then adding 23mL of NaOH solution (2M), heating to 80 ℃, adding 34g of ethyl orthosilicate while stirring, reacting for 6h, filtering, then dissolving in 24mL of methanol, dropwise adding 4mL of concentrated hydrochloric acid, heating to 70 ℃, carrying out acid washing for 18h, filtering, collecting precipitate, washing with methanol and deionized water for multiple times, and drying to obtain 9.8g of mesoporous silica. .
Dissolving 7g of sucrose stearate, 12g of schizonepeta essential oil, 15g of cinnamon essential oil, 3g of rosemary essential oil, 20g of Chinese chestnut flower essential oil, 10g of Xiaoguan smoked leaf essential oil, 3g of galangal essential oil, 10g of parthenium essential oil, 5g of thyme essential oil, 15g of lantana essential oil and 7g of tea tree essential oil in 150mL of 60 ℃ water, then adding 9.8g of mesoporous silicon dioxide, carrying out ultrasonic treatment for 1h, then dropwise adding 40mL of glucan quaternary ammonium salt water solution (0.5g/mL), carrying out ultrasonic treatment for 8min, centrifuging (10000rpm and 10min), washing with deionized water for multiple times, and drying to obtain 125g of nanoparticles.
Example 6
63g of hexadecyl trimethyl ammonium bromide solution is dissolved in 126mL of deionized water, ultrasonic treatment is carried out to completely dissolve the hexadecyl trimethyl ammonium bromide solution, 215mL of NaOH solution (2M) is added, the solution is heated to 85 ℃, 315g of ethyl orthosilicate is added while stirring, the reaction is carried out for 8 hours, filtration is carried out, then the solution is dissolved in 144mL of methanol, 36mL of concentrated hydrochloric acid is dropwise added, the solution is heated to 60 ℃, acid washing is carried out for 24 hours, precipitates are collected by filtration, and after the precipitates are washed for multiple times by methanol and deionized water, drying is carried out to obtain 90g of.
Dissolving 3g of sucrose stearate, 30g of schizonepeta essential oil and 20g of cinnamon essential oil in 80mL of 50 ℃ water, then adding 90g of mesoporous silica, performing ultrasonic treatment for 1h, then dropwise adding 360mL of dextran quaternary ammonium salt aqueous solution (0.5g/mL), performing ultrasonic treatment for 8min, centrifuging (10000rpm, 10min), washing with deionized water for multiple times, and drying to obtain 305g of nanoparticles.
Example 7
40g of plant essential oil nanoparticles of example 1, 7g of jojoba oil, 1g of evening primrose oil, 1.5g of sweet almond oil, 2.7g of wheat germ oil, 2g of pearl barley oil, 0.8g of carrot oil, 6g of glycerin, 4g of butylene glycol, 0.5g of sodium hyaluronate, 1g of β -dextran, 0.5g of allantoin, 1g of purslane extract, 0.3g of ascorbyl tetraisopalmitate, 0.3g of carbomer, 4g of cetostearyl alcohol, 231 g of laureth-231 g, 0.2g of triethanolamine, and the balance of deionized water to 100 g.
The preparation method comprises the following steps: mixing vegetable oil with cetostearyl alcohol and laureth-23, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain an oil phase; mixing deionized water, a thickening agent and glycerol, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain a water phase; adding the oil phase into the water phase while stirring, homogenizing for 2-5 min, and then stirring and cooling; when the temperature is reduced to 40-45 ℃, slowly dripping a pH regulator to regulate the pH to 5-7; finally, adding the plant essential oil nanoparticles, ascorbyl tetraisopalmitate, the humectant and the purslane extract in sequence while stirring; and cooling to room temperature to obtain the slow-release mosquito-repellent emulsion containing the plant essential oil nanoparticles.
Example 8
30g of plant essential oil nanoparticles of example 2, 8g of macadamia nut oil, 9g of glycerol, 0.8g of hexylene glycol, 3.2g of β -dextran, 4g of purslane extract, 0.6g of ascorbyl tetraisopalmitate, 0.02g of seaweed gel, 0.08g of tara gum, 1g of cetostearyl alcohol, 232 g of laureth-232 g, 0.05g of citric acid, and the balance of deionized water to 100 g.
The preparation method comprises the following steps: mixing vegetable oil with cetostearyl alcohol and laureth-23, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain an oil phase; mixing deionized water, a thickening agent and glycerol, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain a water phase; adding the oil phase into the water phase while stirring, homogenizing for 2-5 min, and then stirring and cooling; when the temperature is reduced to 40-45 ℃, slowly dripping a pH regulator to regulate the pH to 5-7; finally, adding the plant essential oil nanoparticles, ascorbyl tetraisopalmitate, the humectant and the purslane extract in sequence while stirring; and cooling to room temperature to obtain the slow-release mosquito-repellent emulsion containing the plant essential oil nanoparticles.
Example 9
20g of plant essential oil nanoparticles of example 3, 4g of macadamia nut oil, 2g of evening primrose oil, 1g of wheat germ oil, 3g of rice bran oil, 1.5g of carrot oil, 12g of glycerol, 2g of niacinamide, 2.5g of purslane extract, 1g of ascorbyl tetraisopalmitate, 0.1g of xanthan gum, 0.15g of gum arabic, 2.5g of cetostearyl alcohol, 233 g of laureth, 0.08g of triethanolamine, 0.05g of citric acid, and the balance of deionized water to 100 g.
The preparation method comprises the following steps: mixing vegetable oil with cetostearyl alcohol and laureth-23, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain an oil phase; mixing deionized water, a thickening agent and glycerol, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain a water phase; adding the oil phase into the water phase while stirring, homogenizing for 2-5 min, and then stirring and cooling; when the temperature is reduced to 40-45 ℃, slowly dripping a pH regulator to regulate the pH to 5-7; finally, adding the plant essential oil nanoparticles, ascorbyl tetraisopalmitate, the humectant and the purslane extract in sequence while stirring; and cooling to room temperature to obtain the slow-release mosquito-repellent emulsion containing the plant essential oil nanoparticles.
Example 10
35g of plant essential oil nanoparticles of example 4, 5g of jojoba oil, 3g of wheat germ oil, 2g of carrot oil, 8g of glycerol, 1g of hexanediol, 1.2g of sodium hyaluronate, 0.8g of nicotinamide, 2g of purslane extract, 0.8g of ascorbyl tetraisopalmitate, 0.4g of tara gum, 2g of cetostearyl alcohol, 232 g of laureth-232 g, 0.1g of triethanolamine, 0.05g of citric acid, and deionized water to make up 100 g.
The preparation method comprises the following steps: mixing vegetable oil with cetostearyl alcohol and laureth-23, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain an oil phase; mixing deionized water, a thickening agent and glycerol, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain a water phase; adding the oil phase into the water phase while stirring, homogenizing for 2-5 min, and then stirring and cooling; when the temperature is reduced to 40-45 ℃, slowly dripping a pH regulator to regulate the pH to 5-7; finally, adding the plant essential oil nanoparticles, ascorbyl tetraisopalmitate, the humectant and the purslane extract in sequence while stirring; and cooling to room temperature to obtain the slow-release mosquito-repellent emulsion containing the plant essential oil nanoparticles.
Example 11
20g of plant essential oil nanoparticles of example 5, 4g of macadamia nut oil, 2g of evening primrose oil, 1g of wheat germ oil, 3g of rice bran oil, 1.5g of carrot oil, 12g of glycerol, 2g of niacinamide, 2.5g of purslane extract, 1g of ascorbyl tetraisopalmitate, 0.5g of xanthan gum, 0.5g of gum arabic, 2.5g of cetostearyl alcohol, 233 g of laureth, 0.08g of triethanolamine, 0.05g of citric acid, and the balance of deionized water to 100 g.
The preparation method comprises the following steps: mixing vegetable oil with cetostearyl alcohol and laureth-23, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain an oil phase; mixing deionized water, a thickening agent and glycerol, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain a water phase; adding the oil phase into the water phase while stirring, homogenizing for 2-5 min, and then stirring and cooling; when the temperature is reduced to 40-45 ℃, slowly dripping a pH regulator to regulate the pH to 5-7; finally, adding the plant essential oil nanoparticles, ascorbyl tetraisopalmitate, the humectant and the purslane extract in sequence while stirring; and cooling to room temperature to obtain the slow-release mosquito-repellent emulsion containing the plant essential oil nanoparticles.
Example 12
40g of plant essential oil nanoparticles of example 6, 7g of jojoba oil, 1g of evening primrose oil, 1.5g of sweet almond oil, 2.7g of wheat germ oil, 2g of pearl barley oil, 0.8g of carrot oil, 6g of glycerin, 4g of butylene glycol, 0.5g of sodium hyaluronate, 1g of β -dextran, 0.5g of allantoin, 1g of purslane extract, 0.3g of ascorbyl tetraisopalmitate, 0.3g of carbomer, 4g of cetostearyl alcohol, 231 g of laureth-231 g, 0.2g of triethanolamine, and the balance of deionized water to 100 g.
The preparation method comprises the following steps: mixing vegetable oil with cetostearyl alcohol and laureth-23, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain an oil phase; mixing deionized water, a thickening agent and glycerol, stirring and heating to 70-85 ℃, and keeping the temperature for 5-10 min to obtain a water phase; adding the oil phase into the water phase while stirring, homogenizing for 2-5 min, and then stirring and cooling; when the temperature is reduced to 40-45 ℃, slowly dripping a pH regulator to regulate the pH to 5-7; finally, adding the plant essential oil nanoparticles, ascorbyl tetraisopalmitate, the humectant and the purslane extract in sequence while stirring; and cooling to room temperature to obtain the slow-release mosquito-repellent emulsion containing the plant essential oil nanoparticles.
Example 13
Mosquito repelling test conditions are as follows: species and strains of test mosquitoes: aedes albopictus (Aedes albopictus), Culex fatigues (Culex pipiens quinquefasciatus) and Culex pallens (Culex pipiens); animals for the test: SD rat; test temperature: 26 +/-1 ℃; relative humidity: 65 plus or minus 5 percent;
test materials: the mosquito repellent emulsions of examples 7-12 further contained Liushen mosquito repellent toilet water and Longliki mosquito repellent toilet water as repellent groups and deionized water as blank groups.
100 test insects were placed in a mosquito cage of 20cm × 20cm × 20cm, and hairs of 2cm × 2cm area were cut from the abdominal area of the rat to expose the skin. After being fixed, the rat is placed in a mosquito cage for 5min, more than 20 test insects which come and stop and fall are qualified in the attack power, and the mosquitoes in the rat and the cage can be used for the test. Fixing SD rat qualified in the attack force test, shearing to expose 2cm × 2cm skin on abdomen, and processing at a rate of 1.5 μ L/cm
2Uniformly smearing the test sample and the reference substance, tightly covering the rest part, placing the rat into a mosquito cage with qualified attack force for 5min after smearing the medicine for 1h, observing whether the mosquito stops falling on the exposed skin, and testing once every hour, wherein the rat fails as long as 1 mosquito stops falling. And repeating the test for 3 times, recording the average effective mosquito repelling time of each sample, and calculating the effective mosquito repelling rate.
The effective mosquito repelling rate is (corresponding to the average number of the stops of the blank preparation-the average number of the stops of the repellent)/the average number of the stops of the corresponding blank preparation is multiplied by 100 percent
TABLE 1 average effective mosquito repellent time (h) for several repellents
| Aedes albopictus | Culex fatigues | Culex pipiens pallens | |
| Mosquito repellent emulsion of example 7 | 13.8*# | 12.3*# | 11.4*# |
| Mosquito repellent emulsion of example 8 | 14.1*# | 12.7*# | 11.0*# |
| Mosquito repellent emulsion of example 9 | 13.6*# | 12.1*# | 11.2*# |
| Mosquito repellent emulsion of example 10 | 14.0*# | 12.5*# | 11.6*# |
| Mosquito repellent emulsion of example 11 | 11.8# | 10.3# | 9.0# |
| Mosquito repellent emulsion of example 12 | 10.5# | 9.1# | 7.9# |
| Liushen mosquito-repellent toilet water | 5.9 | 6.3 | 6.8 |
| Longliki mosquito-repellent toilet water | 5.4 | 6.6 | 7.1 |
Note that # shows that compared with the effect of Liushen mosquito repellent toilet water or Longli mosquito repellent toilet water, the effect is significantly different, and p is less than 0.05;
shows that compared with the effect of the mosquito repellent emulsion in the example 11 or the mosquito repellent emulsion in the example 12, the effect is significantly different, and p is less than 0.05.
TABLE 2 effective repellency Rate (%) of several repellents
The results show that the effective mosquito repelling time and the effective repellent rate of the mosquito repelling emulsion on aedes albopictus, culex fatigues and culex pallens are obviously higher than those of Liushen mosquito repelling toilet water and Longli mosquito repelling toilet water, but the mosquito repelling effect is weakened due to improper formula.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.
Claims (9)
1. The essential oil nanoparticles are characterized by being prepared from the following raw materials in parts by mass:
the essential oil is a composition of schizonepeta essential oil and cinnamon essential oil, wherein the mass ratio of the schizonepeta essential oil to the cinnamon essential oil is 3: 2;
or the essential oil is a composition of rosemary essential oil, Chinese chestnut flower essential oil, corolla parviflora essential oil, galangal essential oil, silver-ash chrysanthemum essential oil, thyme essential oil, lantana camara essential oil and tea tree essential oil, wherein the mass ratio of the rosemary essential oil, the Chinese chestnut flower essential oil, the corolla parviflora essential oil, the galangal essential oil, the parthenolide camara essential oil, the thyme essential oil and the lantana camara essential oil to the tea tree essential oil is 2:18:10:5:20:3:12: 5;
or the essential oil is a composition of schizonepeta essential oil, cinnamon essential oil, rosemary essential oil, Chinese chestnut flower essential oil, corolla fumigated leaf essential oil, galangal essential oil, silvery chrysanthemum essential oil, thyme essential oil, lantana camara essential oil and tea tree essential oil, wherein the mass ratio of the schizonepeta essential oil, the cinnamon essential oil, the rosemary essential oil, the Chinese chestnut flower essential oil, the corolla fumigated leaf essential oil, the galangal essential oil, the silvery chrysanthemum essential oil, the thyme essential oil, the lantana camara essential oil and the tea tree essential oil is 12:15:3:20:10: 5:15: 7;
or the essential oil is a composition of schizonepeta essential oil, Chinese chestnut flower essential oil, corolla vulgaris essential oil, thyme essential oil, lantana camara essential oil and tea tree essential oil, wherein the mass ratio of the schizonepeta essential oil, the Chinese chestnut flower essential oil, the corolla vulgaris essential oil, the parthenium cinerascens essential oil, the thyme essential oil, the lantana camara essential oil and the tea tree essential oil is 10:8:12:10:4:13: 3.
2. The method for preparing the essential oil nanoparticles as claimed in claim 1, which comprises:
step 1: dissolving sucrose stearate and essential oil in water at 50-60 ℃, adding mesoporous silicon dioxide, and performing ultrasonic treatment for 0.5-1 h to prepare a dispersion liquid;
step 2: and dropwise adding a dextran quaternary ammonium salt water solution into the dispersion liquid, performing ultrasonic treatment for 5-10 min, centrifuging, collecting precipitate, washing and drying the precipitate to obtain the essential oil nanoparticles.
3. The method according to claim 2, wherein in step 1:
the mass-volume ratio of the sucrose stearate to the water is (3 g-7 g): (80 mL-150 mL);
the mass-volume ratio of the essential oil to the water is (50 g-100 g): (80 mL-150 mL).
4. The method according to claim 2, wherein the concentration of the quaternary ammonium salt of glucan in the aqueous solution of quaternary ammonium salt of glucan in step 2 is 0.5 g/mL;
the volume ratio of the dispersion liquid to the glucan quaternary ammonium salt water solution is (80-150): (100-200).
5. The use of the essential oil nanoparticles of claim 1 in the preparation of a mosquito repellent product.
6. A mosquito repellent emulsion comprising the essential oil nanoparticles of claim 1, vegetable oil, purslane extract, glycerin, ascorbyl tetraisopalmitate, cetostearyl alcohol, laureth-23, humectant, thickener, pH adjuster, and deionized water;
the humectant is selected from butanediol, hexanediol, sodium hyaluronate, β -dextran, allantoin or nicotinamide.
7. The mosquito repellent emulsion according to claim 6, wherein the mass fraction of each component is as follows:
8. a mosquito repellent emulsion according to claim 6 or 7,
the vegetable oil is selected from jojoba oil, macadamia nut oil, evening primrose oil, sweet almond oil, wheat germ oil, coix seed oil, rice bran oil or carrot oil;
the thickening agent is selected from carbomer, seaweed gum, acacia gum, xanthan gum or Caesalpinia spinosa;
the pH regulator is selected from triethanolamine or citric acid.
9. A preparation method of the mosquito repellent emulsion according to any one of claims 6 to 7, which is characterized by comprising the following steps:
step 1: mixing vegetable oil, cetostearyl alcohol and laureth-23, stirring, heating to 70-85 ℃, stirring, and keeping the temperature for 5-10 min to obtain an oil phase;
step 2: mixing deionized water, a thickening agent and glycerol, stirring, heating to 70-85 ℃, stirring, and keeping the temperature for 5-10 min to obtain a water phase;
and step 3: adding the oil phase into the water phase under the condition of stirring, homogenizing for 2-5 min, stirring and cooling to 40-45 ℃; adjusting the pH value to 5-7, and sequentially adding the essential oil nanoparticles, ascorbyl tetraisopalmitate, humectant and purslane extract according to claim 1; cooling to obtain the mosquito repellent emulsion.
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